CN101037804A - Yttrium erbium ion gadolinium sodium molybdate double-doped laser crystal and preparation method and usage thereof - Google Patents
Yttrium erbium ion gadolinium sodium molybdate double-doped laser crystal and preparation method and usage thereof Download PDFInfo
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- CN101037804A CN101037804A CN 200610067569 CN200610067569A CN101037804A CN 101037804 A CN101037804 A CN 101037804A CN 200610067569 CN200610067569 CN 200610067569 CN 200610067569 A CN200610067569 A CN 200610067569A CN 101037804 A CN101037804 A CN 101037804A
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Abstract
A ytterbium-erbium-ion-double-intermingled gadolinium-natrium molybdate laser crystal and its preparing method and its use, relate to artificial lens field, in particular relate to a laser crystal Ytterbium-erbium-ion-double-intermingled gadolinium-natrium molybdate (Yb3+/Er3+:NaGd(MoO4)2) and its preparing method and its use. Yb3+/Er3+:NaGd(MoO4)2 crystal having high quality and bigger size is produced by the pulling method (Czochralski method) at 1173 DEG C, at the crystal rotational speed of 10-30 turns/minute, under the drawing speed of 0.5-2 mm/hour. The crystal is a novel laser crystal, and can produce the laser output of about 550 nm and 1500 nm wavelengths.
Description
Technical field
The present invention relates to artificial lens and field of crystal growth in the technical field of optoelectronic functional materials.
Background technology
Laser crystals is the operation material of solid statelaser, and it is meant with the crystal to be matrix, by discrete luminescence center absorptive pumping luminous energy and be translated into the luminescent material of laser output.Solid laser working substance is made up of substrate material and active ions, and its various physics and chemical property are mainly by the substrate material decision, and its spectral response curve and fluorescence lifetime etc. are then determined by the level structure of active ions.From nineteen sixty, succeeded in developing since the synthetic ruby pulsed laser, up to now, found hundreds of laser crystalss, but because of a variety of causes, the laser crystals that can really obtain practical application has only ten to plant.
At present, most widely used laser crystals is yttrium aluminum garnet (YAG) crystal of Nd ion doped, and it has various preferably physics and chemical property, and is easy to grow high optical quality, large-sized gem-quality crystal.But it is narrow that it exists spectral line of absorption, is unwell to the shortcoming of carrying out pumping with LD, and the LD pumping will be the developing direction of laser pumping source from now on.
All actively seek various physics, chemical property and mechanical property excellence both at home and abroad at present, and be easy to the high-quality laser crystal material that grows high optical quality, large size and be suitable for the LD pumping.Er
3+The ionic energy level is abundant, and emission wavelength has nine transition passages from seeing near infrared, and wherein the Laser emission of 1.5 μ m and two wave bands of 3.0 μ m is corresponding respectively
4I
13/2→
4I
15/2With
4I
11/2→
4I
15/2Transition between the energy level.1.5 μ m laser is to eye-safe, human cell tissue is to 3.0 μ m laser strong absorption, therefore with Er
3+Ion is that the laser crystals of active ions has a extensive future in fields such as communication and medical treatment.But because Er
3+Reasons such as the weak absorption of ion pair pump light, absorption cross is little, the laser lower level life-span is long, exist shortcomings such as lasing efficiency is low, threshold power height, so in order to obtain gratifying system efficiency, usually the rare earth ion that mixes other is as sensitizing agent, to put forward its laser output efficiency.Mixing Er
3+Mix Yb in the ionic laserable material
3+Ion is as sensitizing agent, Yb
3+Ionic absorption behind the energy of pump light, energy is transferred to Er
3+Ion can reach raising to the assimilated efficiency of pump light and the purpose of reduction laser generation threshold value.And at 600-1000nm zone Yb
3+The absorption band that ion is strong is easy to and business-like LD pumping band coupling.
Summary of the invention
Purpose of the present invention just is to develop a kind of new laser crystals Yb
3+/ Er
3+: NaGd (MoO
4)
2, can directly use photoflash lamp and LD pumping, laser crystal material with higher conversion efficiency.
Yb
3+/ Er
3+: NaGd (MoO
4)
2Crystal belongs to tetragonal system, has I
4 (1)/aThe spacer structure.Wherein erbium ion is as dopant ion, and ytterbium ion is as sensitized ions, replaces the crystallographic site of gadolinium ion simultaneously.When the doping content of erbium is about 1at.%, when the doping content of ytterbium was the 10at.% left and right sides, its fluorescence lifetime (τ) was 4～5ms.Experimental result shows the laser of its exportable 550nm and 1500nm wavelength around, can be used as laser crystals.
Yb
3+/ Er
3+: NaGd (MoO
4)
2Crystal is a kind of compound of congruent melting, adopts Czochralski grown to go out, and presses chemical equation: Na
2CO
3+ Gd
2O
3+ 4MoO
3=2NaGd (MoO
4)
2+ CO
2Ratio claim sample, mixing, compressing tablet, sintering, and Er
2O
3, Yb
2O
3Then pressing desired concn adds.Raw materials usedly be:
| The medicine name | Purity | Producer |
| Er 2O 3 | 99.999％ | Changchun Applied Chemistry Research Inst., Chinese Academy of Sciences |
| Yb 2O 3 | 99.999％ | Changchun Applied Chemistry Research Inst., Chinese Academy of Sciences |
| Gd 2O 3 | 99.999％ | Changchun Applied Chemistry Research Inst., Chinese Academy of Sciences |
| Na 2CO 3 | 99.99％ | Shanghai the May 4th chemical reagent factory |
| MoO 3 | 99.99％ | Shanghai chemical reagents corporation of Chinese Medicine group |
Its main growth conditions is as follows: growth is to carry out in Platinum crucible, under the oxygen-enriched atmosphere (air), the parameter of crystal growth is 1173 ℃ of growth temperatures, pulling speed is 0.5～1.0 millimeter/hour, and 10～30 rev/mins of crystal rotating speeds have grown high-quality Yb
3+/ Er
3+: NaGd (MoO
4)
2Crystal.
With the Yb that grows
3+/ Er
3+: NaGd (MoO
4)
2Crystal has carried out the collection of diffraction data on four-circle diffractometer, structural analysis shows that it belongs to tetragonal system, and spacer is I
4 (1)/a, unit cell parameters is a=b=5.21 , c=11.41 , V=310
3, D
c=5.36g/cm
3
With the Yb that grows
3+/ Er
3+: NaGd (MoO
4)
2Crystal carries out the analytical test of polarization absorption spectrum, fluorescence spectrum and fluorescence lifetime etc., and the result shows: mix 0.75at.%Er
3+And 5.52at.%Yb
3+Yb
3+/ Er
3+: NaGd (MoO
4)
2Crystalline master absorption peak is 3.10cm at 976nm and 1501nm place for the uptake factor of π polarization at the 1501nm place
-1, be 2.67cm for the uptake factor of σ polarization at the 1501nm place
-1In addition, it has strong fluorescence emission peak near wavelength 550nm and 1537nm, and fluorescence lifetime is 4.69ms, because the long crystal of fluorescence lifetime can accumulate more particle at last energy level, has increased energy storage, helps the raising of device output rating and output energy.Therefore, Yb
3+/ Er
3+: NaGd (MoO
4)
2Crystal can obtain the output of more powerful laser, is a kind of high conversion efficiency, low cost, high optical quality and actual application prospect is arranged and the laser crystals of use value.
Yb
3+/ Er
3+: NaGd (MoO
4)
2Crystal can grow superior in quality crystal, fast growth easily with crystal pulling method; The crystalline Vickers' hardness is 334VDH, and hardness is moderate, is convenient to processing; Has good heat-conducting; Good optical characteristics is arranged; Be easy to obtain laser output with flash lamp pumping and LD pumping, laser output wavelength is about 550nm and 1500nm, and this crystal can be used as a kind of laser crystals preferably.
Embodiment
Embodiment 1: the Czochralski grown doping content is 1.0at.%Er
3+And 10at.%Yb
3+Yb
3+/ Er
3+: NaGd (MoO
4)
2Laser crystals.
Will be by the load weighted Na of proportion speed
2CO
3, Gd
2O
3, MoO
3, Er
2O
3, Yb
2O
3Mixed grinding is even, behind the compressing tablet, puts into Φ 80 * 80mm
3Corundum crucible in, in retort furnace in 650 ℃ of solid state reactions 24 hours; After the taking-up, grind compressing tablet again and be warming up to 850 ℃ of reactions 24 hours again.Synthetic good above sample is put into Φ 50 * 40mm
3Platinum crucible in, adopt crystal pulling method, in air atmosphere, growth temperature is 1173 ℃, the crystal rotating speed is 30 rev/mins, pulling rate is under 1 millimeter/hour the situation, to have grown and be of a size of Φ 20 * 37mm
3High-quality Yb
3+/ Er
3+: NaGd (MoO
4)
2Crystal.Er in ICP test shows crystal
3+Ion content is 0.75at.%, Yb
3+Ion content is 5.52at.%.
Claims (4)
1. Yttrium erbium ion gadolinium sodium molybdate double-doped laser crystal, it is characterized in that: this crystalline molecular formula is Yb
3+/ Er
3+: NaGd (MoO
4)
2, doping content is respectively: Er
3+: 0.1at.-5at.%, Yb
3+: 0.5at.-15at.%, belong to tetragonal system, spacer is I
4 (1)/a, unit cell parameters is a=b=5.21 , c=11.41 , V=310
3, D
c=5.36g/cm
3
2. the preparation method of the Yttrium erbium ion gadolinium sodium molybdate double-doped laser crystal of a claim 1 is characterized in that: this crystal by adopting Czochralski grown.
3. preparation method as claimed in claim 2 is characterized in that: described crystal pulling method is with Gd
2O
3, Na
2CO
3, MoO
3, Er
2O
3And Yb
2O
3Be raw material, the parameter of crystal growth is about 1173 ℃ of growth temperatures, and pulling speed is 0.5～1.0 millimeter/hour, and the crystal rotating speed is 10～30 rev/mins.
4. the purposes of the Yttrium erbium ion gadolinium sodium molybdate double-doped laser crystal of a claim 1, it is characterized in that: this crystal is used for solid statelaser as working-laser material.
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|---|---|---|---|
| CN 200610067569 CN101037804A (en) | 2006-03-17 | 2006-03-17 | Yttrium erbium ion gadolinium sodium molybdate double-doped laser crystal and preparation method and usage thereof |
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|---|---|---|---|
| CN 200610067569 CN101037804A (en) | 2006-03-17 | 2006-03-17 | Yttrium erbium ion gadolinium sodium molybdate double-doped laser crystal and preparation method and usage thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101037804A true CN101037804A (en) | 2007-09-19 |
Family
ID=38888969
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|---|---|---|---|
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|---|---|
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Cited By (6)
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|---|---|---|---|---|
| CN102766906A (en) * | 2011-05-05 | 2012-11-07 | 中国科学院福建物质结构研究所 | Erbium ion activated 3-micron wave-band gallate laser crystal and its preparation method |
| CN101457399B (en) * | 2007-12-11 | 2013-01-02 | 中国科学院福建物质结构研究所 | Erbium sodium ion double doped strontium molybdate laser crystal and preparation method thereof |
| CN102877132A (en) * | 2012-10-22 | 2013-01-16 | 中国科学院福建物质结构研究所 | Ytterbium-doped molybdic acid gadolinium barium potassium laser crystal and preparation method thereof |
| CN101588010B (en) * | 2008-05-22 | 2013-03-20 | 中国科学院福建物质结构研究所 | Molybdate laser crystal doped with erbium ions, ytterbium ions and cerium ions and application thereof |
| CN106029833A (en) * | 2014-02-24 | 2016-10-12 | 株式会社Ｇｂｒｙ | Up-conversion phosphor |
| CN108410461A (en) * | 2018-03-09 | 2018-08-17 | 同济大学 | A kind of complex phase tungsten hydrochlorate up-conversion luminescent material and the preparation method and application thereof |
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2006
- 2006-03-17 CN CN 200610067569 patent/CN101037804A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101457399B (en) * | 2007-12-11 | 2013-01-02 | 中国科学院福建物质结构研究所 | Erbium sodium ion double doped strontium molybdate laser crystal and preparation method thereof |
| CN101588010B (en) * | 2008-05-22 | 2013-03-20 | 中国科学院福建物质结构研究所 | Molybdate laser crystal doped with erbium ions, ytterbium ions and cerium ions and application thereof |
| CN102766906A (en) * | 2011-05-05 | 2012-11-07 | 中国科学院福建物质结构研究所 | Erbium ion activated 3-micron wave-band gallate laser crystal and its preparation method |
| CN102877132A (en) * | 2012-10-22 | 2013-01-16 | 中国科学院福建物质结构研究所 | Ytterbium-doped molybdic acid gadolinium barium potassium laser crystal and preparation method thereof |
| CN106029833A (en) * | 2014-02-24 | 2016-10-12 | 株式会社Ｇｂｒｙ | Up-conversion phosphor |
| EP2985332A4 (en) * | 2014-02-24 | 2016-10-26 | Gbry Co Ltd | Up-conversion phosphor |
| CN106029833B (en) * | 2014-02-24 | 2019-06-07 | 株式会社Ｇｂｒｙ | Up-conversion fluorescence body |
| CN108410461A (en) * | 2018-03-09 | 2018-08-17 | 同济大学 | A kind of complex phase tungsten hydrochlorate up-conversion luminescent material and the preparation method and application thereof |
| CN108410461B (en) * | 2018-03-09 | 2021-05-11 | 同济大学 | Complex phase tungsten molybdate up-conversion luminescent material and preparation method and application thereof |
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Open date: 20070919 |